An Ylidic Cp and its Scandium Complexes in Equilibrium,Organometallics

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An Ylidic Cp and its Scandium Complexes in Equilibrium
Organometallics ( IF 2.5 ) Pub Date : 2021-08-23 , DOI: 10.1021/acs.organomet.1c00351
Fabio Mazzotta ₁ , Doris Kunz ₁

Affiliation

Scandium complexes bearing a C-ylidic, electron-deficient Cp ligand are presented by starting from [ScCl₃(thf)₃]. As ylidic ligands do not require salt metathesis, the coordination of the Cp ligand is realized by mere substitution of the tetrahydrofuran ligands. In acetonitrile an equilibrium among the free ligand, the half-sandwich complex, and the cationic metallocene with its tetrachloridoscandate counterion is observed via NMR spectroscopy. This equilibrium is fully confirmed by ¹H and ⁴⁵Sc NMR EXSY experiments. In the absence of coordinating solvents, the selective formation of all compounds of the equilibrium has been achieved, and the structures have been confirmed by NMR spectroscopy and X-ray structure analysis. Especially ⁴⁵Sc NMR spectroscopy reveals signals with characteristic chemical shifts for the half-sandwich complex and the metallocene. With scandium triflate the corresponding scandocene is also accessible.

中文翻译：

平衡态的 Ylidic Cp 及其钪配合物

从[ScCl ₃ (thf) ₃ ]开始呈现带有C-叶立克、缺电子Cp配体的钪配合物。由于叶立德配体不需要盐复分解，Cp 配体的配位仅通过四氢呋喃配体的取代来实现。在乙腈中，游离配体、半夹心络合物和阳离子茂金属及其四氯化钪酸盐反离子之间的平衡通过 NMR 光谱观察到。这种平衡由¹ H 和⁴⁵Sc NMR EXSY 实验。在没有配位溶剂的情况下，实现了所有平衡化合物的选择性形成，其结构已通过核磁共振光谱和X射线结构分析得到证实。特别是⁴⁵ Sc NMR 光谱揭示了具有半夹心配合物和茂金属的特征化学位移的信号。使用三氟甲磺酸钪也可以使用相应的扫描二碳世。

更新日期：2021-09-13

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